KR20190131618A - Thick-film pastes containing lead- and tellurium-oxides, and their use in the manufacture of semiconductor devices - Google Patents
Thick-film pastes containing lead- and tellurium-oxides, and their use in the manufacture of semiconductor devices Download PDFInfo
- Publication number
- KR20190131618A KR20190131618A KR1020197034102A KR20197034102A KR20190131618A KR 20190131618 A KR20190131618 A KR 20190131618A KR 1020197034102 A KR1020197034102 A KR 1020197034102A KR 20197034102 A KR20197034102 A KR 20197034102A KR 20190131618 A KR20190131618 A KR 20190131618A
- Authority
- KR
- South Korea
- Prior art keywords
- paste
- tellurium
- oxide
- thick film
- lead
- Prior art date
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Images
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/00—Energy generation through renewable energy sources
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Abstract
본 발명은 하나 이상의 절연 층을 갖는 태양 전지 디바이스의 전면을 인쇄하기 위한 후막 페이스트를 제공한다. 후막 페이스트는 유기 매질 내에 분산된 전기 전도성 금속, 및 납-텔루륨-산화물을 포함한다.The present invention provides a thick film paste for printing the front side of a solar cell device having one or more insulating layers. The thick film paste includes an electrically conductive metal dispersed in an organic medium, and lead-tellurium-oxide.
Description
본 발명은 하나 이상의 절연 층을 갖는 태양 전지 디바이스의 전면을 인쇄하기 위한 후막 페이스트를 제공한다. 후막 페이스트는 유기 매질 내에 분산된 전기 전도성 금속, 및 납-텔루륨-산화물을 포함한다.The present invention provides a thick film paste for printing the front side of a solar cell device having one or more insulating layers. The thick film paste includes an electrically conductive metal dispersed in an organic medium, and lead-tellurium-oxide.
p형 베이스(base)를 갖는 종래의 태양 전지 구조물은 전형적으로 전지의 전면 (태양측 면(sun side)) 상에 있는 음극과 후면 상에 있는 양극을 갖는다. 반도체 본체의 p-n 접합부 상으로 떨어지는 적합한 파장의 방사선은 정공-전자 쌍 전하 담체를 생성하기 위한 외부 에너지원으로서의 역할을 한다. 이들 전자-정공 쌍 전하 담체는 p-n 반도체 접합부에 의해 발생된 전기장에서 이동하고, 반도체의 표면에 적용된 금속 접촉 또는 전도성 그리드에 의해 수합된다. 발생된 전류는 외부 회로로 흐른다.Conventional solar cell structures with a p-type base typically have a cathode on the front side (sun side) of the cell and an anode on the back side. Appropriate wavelengths of radiation falling onto the p-n junction of the semiconductor body serve as an external energy source for generating hole-electron pair charge carriers. These electron-hole pair charge carriers migrate in the electric field generated by the p-n semiconductor junction and are collected by a metal contact or conductive grid applied to the surface of the semiconductor. The generated current flows to the external circuit.
전도성 페이스트 (또는 잉크(ink)라고도 함)는 전형적으로 전도성 그리드 또는 금속 접촉을 형성하는 데 사용된다. 전도성 페이스트는 전형적으로 유리 프릿(glass frit), 전도성 화학종 (예를 들어, 은 입자), 및 유기 매질을 포함한다. 금속 접촉을 형성하기 위해, 전도성 페이스트는 그리드 선 또는 다른 패턴으로서 기판 위로 인쇄된 다음, 소성(fire)되고 그 동안에 전기적 접촉이 그리드 선과 반도체 기판 사이에 형성된다.Conductive paste (also called ink) is typically used to form conductive grids or metal contacts. Conductive pastes typically include glass frit, conductive species (eg silver particles), and organic media. To form the metal contact, the conductive paste is printed onto the substrate as grid lines or other patterns, then fired, during which electrical contact is formed between the grid lines and the semiconductor substrate.
그러나, 결정질 규소 PV 전지는 전형적으로 질화규소, 산화티타늄 또는 산화규소와 같은 반사방지 코팅으로 코팅되어 광 흡착을 촉진시키며, 이는 전지의 효율을 증가시킨다. 그러한 반사방지 코팅은 또한 절연체로서 작용하며 이는 기판으로부터 금속 접촉으로의 전자의 흐름을 손상시킨다. 이러한 문제점을 극복하기 위해, 전도성 잉크는 반도체 기판과 전기적 접촉을 갖는 금속 접촉을 형성하기 위해 소성 동안에 반사방지 코팅에 침투해야 할 것이다. 금속 접촉과 기판 사이에서 강한 결합을 형성하는 것이 또한 바람직하다.However, crystalline silicon PV cells are typically coated with an antireflective coating such as silicon nitride, titanium oxide or silicon oxide to promote light adsorption, which increases the efficiency of the cell. Such antireflective coatings also act as insulators, which impair the flow of electrons from the substrate to the metal contacts. To overcome this problem, the conductive ink will have to penetrate the antireflective coating during firing to form metal contacts with electrical contact with the semiconductor substrate. It is also desirable to form a strong bond between the metal contact and the substrate.
소성 시, 반사방지 코팅에 침투하고 기판과 강한 결합을 형성하는 능력은 전도성 잉크의 조성 및 소성 조건에 크게 좌우한다. PV 전지 성능의 주요한 측정인 효율은 소성된 전도성 잉크와 기판 사이에 형성되는 전기적 접촉의 질에 의해 또한 영향을 받는다.Upon firing, the ability to penetrate the antireflective coating and form strong bonds with the substrate is highly dependent on the composition of the conductive ink and the firing conditions. Efficiency, which is a major measure of PV cell performance, is also influenced by the quality of electrical contact formed between the calcined conductive ink and the substrate.
효율이 양호한 PV 전지를 제조하기 위한 경제적인 방법을 제공하기 위해서는, 반사방지 코팅에 침투하고 반도체 기판과 양호한 전기적 접촉을 제공하기 위해 저온에서 소성될 수 있는 후막 페이스트 조성물이 필요하다.In order to provide an economical way to make good PV cells, there is a need for thick film paste compositions that can penetrate antireflective coatings and be baked at low temperatures to provide good electrical contact with the semiconductor substrate.
본 발명의 한 측면은:One aspect of the invention is:
a) 조성물 내 총 고형물을 기준으로 85 중량% 내지 99.5 중량%의 전기 전도성 금속 또는 그의 유도체;a) 85 to 99.5 weight percent of the electrically conductive metal or derivative thereof, based on the total solids in the composition;
b) 고형물을 기준으로 0.5 중량% 내지 15 중량%의 납-텔루륨-산화물 (여기서, 납-텔루륨-산화물의 납 대 텔루륨의 몰 비는 5/95 내지 95/5임); 및b) 0.5 wt% to 15 wt% lead-tellurium-oxide based on solids, wherein the molar ratio of lead to tellurium of lead-tellurium-oxide is 5/95 to 95/5; And
c) 유기 매질을 포함하는 후막 페이스트 조성물이다.c) a thick film paste composition comprising an organic medium.
본 발명의 또 다른 측면은:Another aspect of the invention is:
(a) 반도체 기판 위에 침착된 하나 이상의 절연막을 포함하는 반도체 기판을 제공하는 단계;(a) providing a semiconductor substrate comprising one or more insulating films deposited over the semiconductor substrate;
(b) 하나 이상의 절연막 위로 후막 페이스트 조성물을 도포하여 계층화된 구조물을 형성하는 단계,(b) applying the thick film paste composition over the one or more insulating films to form a layered structure,
(여기서, 후막 페이스트 조성물은:Wherein the thick film paste composition is:
i) 조성물 내 총 고형물을 기준으로 85 중량% 내지 99.5 중량%의 전기 전도성 금속 또는 그의 유도체;i) 85 to 99.5 weight percent of the electrically conductive metal or derivative thereof, based on the total solids in the composition;
ii) 고형물을 기준으로 0.5 중량% 내지 15 중량%의 납-텔루륨-산화물 (여기서, 납-텔루륨-산화물의 납 대 텔루륨의 몰 비는 5/95 내지 95/5임); 및ii) 0.5% to 15% by weight of lead-tellurium-oxide based on solids, wherein the molar ratio of lead to tellurium of lead-tellurium-oxide is 5/95 to 95/5; And
iii) 유기 매질을 포함함); 및iii) an organic medium); And
(c) 반도체 기판, 하나 이상의 절연막, 및 후막 페이스트를 소성시키고, 하나 이상의 절연 층과 접촉하고 반도체 기판과 전기적 접촉하는 전극을 형성하는 단계를 포함하는, 방법이다.(c) firing the semiconductor substrate, the one or more insulating films, and the thick film paste, and forming an electrode in contact with the one or more insulating layers and in electrical contact with the semiconductor substrate.
본 발명의 또 다른 측면은:Another aspect of the invention is:
a) 반도체 기판;a) a semiconductor substrate;
b) 반도체 기판 위의 하나 이상의 절연 층; 및b) one or more insulating layers over the semiconductor substrate; And
c) 하나 이상의 절연 층과 접촉하고 반도체 기판과 전기적 접촉하는 전극 (전극은 전기 전도성 금속 및 납-텔루륨-산화물을 포함함)을 포함하는 물품이다.c) an article comprising an electrode in contact with at least one insulating layer and in electrical contact with the semiconductor substrate, the electrode comprising an electrically conductive metal and lead-tellurium-oxide.
<도 1>
도 1은 반도체 디바이스의 제조를 도시하는 공정 흐름도이다. 도 1에 도시된 도면 부호는 아래에 설명되어 있다.
10: p형 규소 기판
20: n형 확산층
30: 절연막
40: p+ 층(후면 전계, BSF)
60: 후면 위에 침착된 알루미늄 페이스트
61: 알루미늄 후면 전극 (후면 알루미늄 페이스트를 소성시켜서 수득됨)
70: 후면 위에 침착된 은 또는 은/알루미늄 페이스트.
71: 은 또는 은/알루미늄 후면 전극 (후면 은 페이스트를 소성시킴으로써 수득됨)
500: 전면 위에 침착된 후막 페이스트
501: 전면 전극 (후막 페이스트를 소성시킴으로써 형성됨)<Figure 1>
1 is a process flow diagram illustrating the manufacture of a semiconductor device. Reference numerals shown in FIG. 1 are described below.
10: p-type silicon substrate
20: n-type diffusion layer
30: insulating film
40: p + layer (rear field, BSF)
60: aluminum paste deposited on the back
61: aluminum back electrode (obtained by firing rear aluminum paste)
70: silver or silver / aluminum paste deposited on the back side.
71: silver or silver / aluminum back electrode (obtained by firing back silver paste)
500: thick film paste deposited on the front surface
501: front electrode (formed by firing thick film paste)
태양광 발전 광기전력 시스템은 화석 연료에 대한 요구를 감소시킨다는 점에서 환경 친화적인 것으로 여겨진다.Solar photovoltaic systems are considered environmentally friendly in that they reduce the need for fossil fuels.
본 발명은 전기적 성능이 개선된 광기전력 디바이스를 제조하는 데 사용될 수 있는 조성물을 제공한다. 후막 페이스트 조성물은:The present invention provides compositions that can be used to make photovoltaic devices with improved electrical performance. The thick film paste composition is:
a) 조성물 내 총 고형물을 기준으로 85 중량% 내지 99.5 중량%의 전기 전도성 금속 또는 그의 유도체;a) 85 to 99.5 weight percent of the electrically conductive metal or derivative thereof, based on the total solids in the composition;
b) 고형물을 기준으로 0.5 중량% 내지 15 중량%의 납-텔루륨-산화물 (여기서, 납-텔루륨-산화물의 납 대 텔루륨의 몰 비는 5/95 내지 95/5임); 및b) 0.5 wt% to 15 wt% lead-tellurium-oxide based on solids, wherein the molar ratio of lead to tellurium of lead-tellurium-oxide is 5/95 to 95/5; And
c) 유기 매질을 포함한다.c) organic media.
본 명세서에서 정의된 바와 같이, 유기 매질은 후막 페이스트 조성물을 포함하는 고형물의 일부인 것으로 여겨지지 않는다.As defined herein, the organic medium is not considered to be part of the solid comprising the thick film paste composition.
전기 전도성 금속Electrically conductive metal
전기 전도성 금속은 은, 구리 및 팔라듐으로 이루어진 군으로부터 선택된다. 전기 전도성 금속은 박편(flake) 형태, 구 형태, 과립 형태, 결정 형태, 분말 형태 또는 기타 불규칙한 형태 및 그의 혼합물일 수 있다. 전기 전도성 금속은 콜로이드 현탁액에서 제공될 수 있다.The electrically conductive metal is selected from the group consisting of silver, copper and palladium. The electrically conductive metal may be in flake form, sphere form, granule form, crystalline form, powder form or other irregular form and mixtures thereof. The electrically conductive metal may be provided in a colloidal suspension.
금속이 은일 때, 이는 은 금속, 은 유도체, 또는 그의 혼합물의 형태일 수 있다. 예시적인 유도체는: 예를 들어, 은 합금, 산화은 (Ag2O), 은 염, 예컨대 AgCl, AgNO3, AgOOCCH3 (은 아세테이트), AgOOCF3 (은 트라이플루오로아세테이트), 또는 은 오르토포스페이트, Ag3PO4를 포함한다. 다른 후막 페이스트 성분들과 융화성인 다른 형태의 은이 또한 사용될 수 있다.When the metal is silver, it may be in the form of silver metal, silver derivatives, or mixtures thereof. Exemplary derivatives include, for example, silver alloys, silver oxide (Ag 2 O), silver salts such as AgCl, AgNO 3 , AgOOCCH 3 (silver acetate), AgOOCF 3 (silver trifluoroacetate), or silver orthophosphate, Ag 3 PO 4 . Other forms of silver that are compatible with other thick film paste components may also be used.
한 실시 양태에서, 전기 전도성 금속 또는 그의 유도체는 약 85 중량% 내지 약 99.5 중량%의, 후막 페이스트 조성물의 고형물 성분이다. 추가의 실시 양태에서, 전기 전도성 금속 또는 그의 유도체는 약 90 중량% 내지 약 95 중량%의, 후막 페이스트 조성물의 고형물 성분이다.In one embodiment, the electrically conductive metal or derivative thereof is about 85% to about 99.5% by weight solids component of the thick film paste composition. In further embodiments, the electrically conductive metal or derivative thereof is from about 90% to about 95% by weight solids component of the thick film paste composition.
한 실시 양태에서, 후막 페이스트 조성물의 고형물 부분은 약 85 중량% 내지 약 99.5 중량%의 구형 은 입자를 포함한다. 한 실시 양태에서, 후막 페이스트 조성물의 고형물 부분은 약 85 중량% 내지 약 90 중량%의 은 입자 및 약 1 중량% 내지 약 9.5 중량%의 은 박편을 포함한다.In one embodiment, the solid portion of the thick film paste composition comprises from about 85 wt% to about 99.5 wt% spherical silver particles. In one embodiment, the solid portion of the thick film paste composition comprises about 85 wt% to about 90 wt% silver particles and about 1 wt% to about 9.5 wt% silver flakes.
한 실시 양태에서, 후막 페이스트 조성물은 전기 전도성인 코팅된 은 입자를 포함한다. 적합한 코팅은 포스페이트 및 계면활성제를 포함한다. 적합한 계면활성제에는 폴리에틸렌옥사이드, 폴리에틸렌글리콜, 벤조트라이아졸, 폴리(에틸렌글리콜)아세트산, 라우르산, 올레산, 카프르산, 미리스트산, 리놀산, 스테아르산, 팔미트산, 스테아레이트 염, 팔미테이트 염, 및 그의 혼합물이 포함된다. 염 반대 이온은 암모늄, 나트륨, 칼륨, 및 그의 혼합물일 수 있다.In one embodiment, the thick film paste composition comprises coated silver particles that are electrically conductive. Suitable coatings include phosphates and surfactants. Suitable surfactants include polyethylene oxide, polyethylene glycol, benzotriazole, poly (ethylene glycol) acetic acid, lauric acid, oleic acid, capric acid, myristic acid, linoleic acid, stearic acid, palmitic acid, stearate salt, palmitate Salts, and mixtures thereof. Salt counter ions may be ammonium, sodium, potassium, and mixtures thereof.
은의 입자 크기는 어떠한 특정 제한도 받지 않는다. 한 실시 양태에서, 평균 입자 크기는 0.5 미크론 내지 10 미크론이고; 또 다른 실시 양태에서, 평균 입자 크기는 1 미크론 내지 5 미크론이다. 본 명세서에서 사용되는 바와 같이, "입자 크기" 또는 "D50"은 "평균 입자 크기"를 의미하고자 하고; "평균 입자 크기"는 50% 부피 분포 크기를 의미한다. 부피 분포 크기는 마이크로트랙(Microtrac) 입자 크기 분석기를 사용한 레이저 회절 및 분산 방법에 의해 측정될 수 있다.The particle size of silver is not subject to any particular limitation. In one embodiment, the average particle size is from 0.5 microns to 10 microns; In yet another embodiment, the average particle size is 1 micron to 5 microns. As used herein, "particle size" or "D50" is intended to mean "average particle size"; "Average particle size" means 50% volume distribution size. The volume distribution size can be measured by laser diffraction and dispersion methods using a Microtrac particle size analyzer.
납-텔루륨-산화물Lead-tellurium-oxide
납-텔루륨-산화물 (Pb-Te-O)은 TeO2 및 납 산화물 분말을 혼합하고, 분말 혼합물을 공기 또는 산소-함유 분위기에서 가열하여 용융물을 형성하고, 용융물을 급랭시키고, 급랭된 물질을 연삭 및 볼-분쇄하고, 분쇄된 물질을 스크리닝하여 원하는 입자 크기를 갖는 분말을 제공함으로써 제조될 수 있다. 납 산화물 분말은: PbO, Pb3O4, 및 PbO2로 이루어진 군으로부터 선택되는 하나 이상의 성분을 포함할 수 있다. 납 및 텔루륨 산화물의 혼합물을 소성시키는 단계는 전형적으로 800℃ 내지 1200℃의 피크 온도로 수행된다. 용융 혼합물을 예를 들어 스테인리스 강 압반 상에서, 또는 역회전(counter-rotating) 스테인리스 강 롤러들 사이에서 급랭시켜 두꺼운 소판(platelet)을 형성할 수 있다. 생성 소판은 분쇄되어 분말을 형성할 수 있다. 전형적으로, 분쇄된 분말은 0.1 미크론 내지 3.0 미크론의 D50을 갖는다. 한 실시 양태에서, 이러한 방식으로 형성된 Pb-Te-O는 적어도 부분적으로 결정질일 수 있다.Lead-tellurium-oxide (Pb-Te-O) mixes TeO 2 and lead oxide powders and heats the powder mixture in an air or oxygen-containing atmosphere to form a melt, quench the melt and quench the quenched material. It can be prepared by grinding and ball-grinding and screening the ground material to provide a powder with the desired particle size. The lead oxide powder may comprise one or more components selected from the group consisting of: PbO, Pb 3 O 4 , and PbO 2 . Firing the mixture of lead and tellurium oxide is typically carried out at a peak temperature of 800 ° C to 1200 ° C. The molten mixture may be quenched, for example, on a stainless steel platen or between counter-rotating stainless steel rollers to form thick platelets. The resulting platelets can be ground to form a powder. Typically, the milled powder has a D 50 of 0.1 micron to 3.0 microns. In one embodiment, Pb-Te-O formed in this manner may be at least partially crystalline.
전형적으로, PbO 및 TeO2 분말의 혼합물은 조합된 분말을 기준으로 5 몰% 내지 95 몰%의 납 산화물 및 5 몰% 내지 95 몰%의 텔루륨 산화물을 포함한다. 한 실시 양태에서, PbO 및 TeO2 분말의 혼합물은 조합된 분말을 기준으로 30 몰% 내지 85 몰%의 납 산화물 및 15 몰% 내지 70 몰%의 텔루륨 산화물을 포함한다. 또 다른 실시 양태에서, PbO 및 TeO2 분말의 혼합물은 조합된 분말을 기준으로 30 몰% 내지 65 몰%의 납 산화물 및 35 몰% 내지 70 몰%의 텔루륨 산화물을 포함한다.Typically, the mixture of PbO and TeO 2 powders comprises 5 mol% to 95 mol% lead oxide and 5 mol% to 95 mol% tellurium oxide, based on the combined powder. In one embodiment, the mixture of PbO and TeO 2 powders comprises 30 mol% to 85 mol% lead oxide and 15 mol% to 70 mol% tellurium oxide based on the combined powder. In another embodiment, the mixture of PbO and TeO 2 powders comprises 30 mol% to 65 mol% lead oxide and 35 mol% to 70 mol% tellurium oxide based on the combined powder.
일부 실시 양태에서, PbO 및 TeO2 분말의 혼합물은 하나 이상의 다른 금속 화합물을 추가로 포함한다. 적합한 다른 금속 화합물은 TiO2, LiO2, B2O3, PbF2, SiO2, Na2O, K2O, Rb2O, Cs2O, Al2O3, MgO, CaO, SrO, BaO, V2O5, ZrO2, MoO3, Mn2O3, Ag2O, ZnO, Ga2O3, GeO2, In2O3, SnO2, Sb2O3, Bi2O3, BiF3, P2O5, CuO, NiO, Cr2O3, Fe2O3, CoO, Co2O3, 및 CeO2를 포함한다.In some embodiments, the mixture of PbO and TeO 2 powders further comprises one or more other metal compounds. Other suitable metal compounds are TiO 2 , LiO 2 , B 2 O 3 , PbF 2 , SiO 2 , Na 2 O, K 2 O, Rb 2 O, Cs 2 O, Al 2 O 3 , MgO, CaO, SrO, BaO , V 2 O 5 , ZrO 2 , MoO 3 , Mn 2 O 3 , Ag 2 O, ZnO, Ga 2 O 3 , GeO 2 , In 2 O 3 , SnO 2 , Sb 2 O 3 , Bi 2 O 3 , BiF 3 , P 2 O 5 , CuO, NiO, Cr 2 O 3 , Fe 2 O 3 , CoO, Co 2 O 3 , and CeO 2 .
표 1 및 2는 납-텔루륨 산화물을 제조하는 데 사용될 수 있는 PbO, TeO2 및 다른 선택적인 금속 화합물을 함유하는 분말 혼합물의 일부 예를 열거한다. 이 목록은 예시적인 것이고 제한적인 것은 아니다.Tables 1 and 2 list some examples of powder mixtures containing PbO, TeO 2 and other optional metal compounds that can be used to prepare lead-tellurium oxide. This list is illustrative and not restrictive.
따라서, 본 명세서에서 사용되는 바와 같이, 용어 "Pb-Te-O"는 Si, Sn, Li, Ti, Ag, Na, K, Rb, Cs, Ge, Ga, In, Ni, Zn, Ca, Mg, Sr, Ba, Se, Mo, W, Y, As, La, Nd, Co, Pr, Gd, Sm, Dy, Eu, Ho, Yb, Lu, Bi, Ta, V, Fe, Hf, Cr, Cd, Sb, Bi, F, Zr, Mn, P, Cu, Ce, 및 Nb로 이루어진 군으로부터 선택되는 하나 이상의 구성원의 산화물을 함유하는 금속 산화물을 또한 포함할 수 있다.Thus, as used herein, the term "Pb-Te-O" refers to Si, Sn, Li, Ti, Ag, Na, K, Rb, Cs, Ge, Ga, In, Ni, Zn, Ca, Mg , Sr, Ba, Se, Mo, W, Y, As, La, Nd, Co, Pr, Gd, Sm, Dy, Eu, Ho, Yb, Lu, Bi, Ta, V, Fe, Hf, Cr, Cd And may also include metal oxides containing oxides of one or more members selected from the group consisting of Sb, Bi, F, Zr, Mn, P, Cu, Ce, and Nb.
유기 매질Organic medium
후막 페이스트 조성물의 무기 성분은 인쇄에 적합한 주도(consistency) 및 리올로지(rheology)를 갖는 점성 페이스트를 형성하도록 유기 매질과 혼합된다. 매우 다양한 불활성 점성 물질이 유기 매질로서 사용될 수 있다. 유기 매질은 페이스트의 제조, 선적 및 보관 동안, 뿐만 아니라 스크린 인쇄 공정 동안 인쇄 스크린 상에서 무기 성분이 충분한 정도의 안정성을 가지고 분산될 수 있는 것일 수 있다.The inorganic component of the thick film paste composition is mixed with the organic medium to form a viscous paste with consistency and rheology suitable for printing. A wide variety of inert viscous materials can be used as the organic medium. The organic medium may be one in which the inorganic components can be dispersed with a sufficient degree of stability during the manufacture, shipping and storage of the paste, as well as during the screen printing process.
적합한 유기 매질은 고형물의 안정한 분산, 스크린 인쇄를 위한 적합한 점도 및 요변성(thixotropy), 기판 및 페이스트 고형물의 적합한 습윤성, 양호한 건조 속도, 및 양호한 소성 특성을 제공하는 리올로지 특성을 갖는다. 유기 매질은 증점제, 안정화제, 계면활성제, 및/또는 다른 일반적인 첨가제를 함유할 수 있다. 유기 매질은 용매(들) 중 중합체(들)의 용액일 수 있다. 적합한 중합체에는 에틸 셀룰로오스, 에틸 하이드록시에틸 셀룰로오스, 나무 로진, 에틸 셀룰로오스와 페놀계 수지의 혼합물, 저급 알코올의 폴리메트아크릴레이트, 및 에틸렌 글리콜 모노아세테이트의 모노부틸 에테르가 포함된다. 적합한 용매에는 알파- 또는 베타-테르피네올과 같은 테르펜, 또는 그와 기타 용매, 예를 들어, 등유, 다이부틸프탈레이트, 부틸 카르비톨, 부틸 카르비톨 아세테이트, 헥실렌 글리콜 및 비등점이 150℃ 초과인 알코올, 및 알코올 에스테르와의 혼합물이 포함된다. 다른 적합한 유기 매질 성분에는 비스(2-(2-부톡시에톡시)에틸 아디페이트, 이염기성 에스테르, 예컨대, DBE, DBE-2, DBE-3, DBE-4, DBE-5, DBE-6, DBE-9, 및 DBE 1B, 옥틸 에폭시 탈레이트, 아이소테트라데칸올, 및 수소화된 로진의 펜타에리트리톨 에스테르가 포함된다. 유기 매질은 또한 후막 페이스트 조성물을 기판에 도포한 후의 신속한 경화를 촉진시키기 위해 휘발성 액체를 포함할 수 있다.Suitable organic media have rheological properties that provide stable dispersion of solids, suitable viscosity and thixotropy for screen printing, suitable wettability of substrate and paste solids, good drying speed, and good firing properties. The organic medium may contain thickeners, stabilizers, surfactants, and / or other common additives. The organic medium may be a solution of polymer (s) in solvent (s). Suitable polymers include ethyl cellulose, ethyl hydroxyethyl cellulose, wood rosin, mixtures of ethyl cellulose and phenolic resins, polymethacrylates of lower alcohols, and monobutyl ethers of ethylene glycol monoacetate. Suitable solvents include terpenes such as alpha- or beta-terpineol, or other solvents such as kerosene, dibutylphthalate, butyl carbitol, butyl carbitol acetate, hexylene glycol and boiling points above 150 ° C. Alcohols, and mixtures with alcohol esters. Other suitable organic medium components include bis (2- (2-butoxyethoxy) ethyl adipate, dibasic esters such as DBE, DBE-2, DBE-3, DBE-4, DBE-5, DBE-6, Pentaerythritol esters of DBE-9, and DBE 1B, octyl epoxy talate, isotetracananol, and hydrogenated rosin The organic medium is also used to promote rapid curing after application of the thick film paste composition to the substrate. Volatile liquids.
후막 페이스트 조성물 중 유기 매질의 최적량은 페이스트의 도포 방법 및 사용되는 특정 유기 매질에 따라 좌우된다. 전형적으로, 후막 페이스트 조성물은 70 중량% 내지 95 중량%의 무기 성분 및 5 중량% 내지 30 중량%의 유기 매질을 함유한다.The optimum amount of organic medium in the thick film paste composition depends on the method of applying the paste and the particular organic medium used. Typically, thick film paste compositions contain from 70% to 95% by weight of inorganic components and from 5% to 30% by weight of organic medium.
유기 매질이 중합체를 포함한다면, 유기 조성물은 8 중량% 내지 15 중량%의 중합체를 포함할 수 있다.If the organic medium comprises a polymer, the organic composition may comprise 8 wt% to 15 wt% polymer.
후막 페이스트 조성물의 제조Preparation of Thick Film Paste Compositions
한 실시 양태에서, 후막 페이스트 조성물은 전도성 금속 분말, Pb-Te-O 분말, 및 유기 매질을 임의의 순서대로 혼합하여 제조될 수 있다. 일부 실시 양태에서, 무기 물질들을 먼저 혼합하고, 이어서 이들을 유기 매질에 첨가한다. 필요하다면 용매를 첨가하여 점도를 조정할 수 있다. 고 전단을 제공하는 혼합 방법이 유용할 수 있다.In one embodiment, the thick film paste composition can be prepared by mixing the conductive metal powder, the Pb-Te-O powder, and the organic medium in any order. In some embodiments, the inorganic materials are first mixed and then added to the organic medium. If necessary, the viscosity can be adjusted by adding a solvent. Mixing methods that provide high shear may be useful.
본 발명의 다른 측면은:Another aspect of the invention is:
a) 반도체 기판의 하나 이상의 표면 위로 침착된 하나 이상의 절연막을 포함하는 반도체 기판을 제공하는 단계;a) providing a semiconductor substrate comprising at least one insulating film deposited over at least one surface of the semiconductor substrate;
(b) 하나 이상의 절연막의 적어도 일부분 위에 후막 페이스트 조성물을 도포하여, 계층화된 구조물을 형성하는 단계 (여기서, 후막 페이스트 조성물은:(b) applying the thick film paste composition over at least a portion of the one or more insulating films to form a layered structure, wherein the thick film paste composition comprises:
i) 조성물 내 총 고형물을 기준으로 85 중량% 내지 99.5 중량%의 전기 전도성 금속 또는 그의 유도체;i) 85 to 99.5 weight percent of the electrically conductive metal or derivative thereof, based on the total solids in the composition;
ii) 고형물을 기준으로 0.5 중량% 내지 15 중량%의 납-텔루륨-산화물 (여기서, 납-텔루륨-산화물의 납 대 텔루륨의 몰 비는 5/95 내지 95/5임); 및ii) 0.5% to 15% by weight of lead-tellurium-oxide based on solids, wherein the molar ratio of lead to tellurium of lead-tellurium-oxide is 5/95 to 95/5; And
iii) 유기 매질을 포함함); 및iii) an organic medium); And
(c) 반도체 기판, 하나 이상의 절연막, 및 후막 페이스트를 소성시키고, 하나 이상의 절연 층과 접촉하고 반도체 기판과 전기적 접촉하는 전극을 형성하는 단계를 포함하는, 방법이다.(c) firing the semiconductor substrate, the one or more insulating films, and the thick film paste, and forming an electrode in contact with the one or more insulating layers and in electrical contact with the semiconductor substrate.
한 실시 양태에서, 반도체 디바이스는 접합부-갖는 반도체 기판 및 그의 주요 표면 상에 형성된 질화규소 절연막을 포함하는 물품으로부터 제조된다. 방법은, 절연 층에 침투하는 능력을 갖는 후막 페이스트 조성물을 예정된 모양 및 두께로 그리고 예정된 위치에서 절연막 위로 도포 (예를 들어, 코팅 또는 스크린-인쇄)하고 그런 다음 소성시켜 후막 페이스트 조성물이 절연막과 반응하고 절연막에 침투하여 규소 기판과 전기적 접촉할 수 있게 하는 단계를 포함한다.In one embodiment, a semiconductor device is made from an article comprising a junction-bearing semiconductor substrate and a silicon nitride insulating film formed on its major surface. The method involves applying (eg, coating or screen-printing) a thick film paste composition having the ability to penetrate the insulating layer over a dielectric film in a predetermined shape and thickness and at a predetermined location and then firing so that the thick film paste composition reacts with the insulating film. And penetrating the insulating film to make electrical contact with the silicon substrate.
이 방법의 한 실시 양태는 도 1에 예시되어 있다.One embodiment of this method is illustrated in FIG. 1.
도 1(a)는 단일-결정 규소 또는 다중-결정질 규소 p-형 기판(10)을 도시한다.1 (a) shows a single-crystalline silicon or multi-crystalline silicon p-
도 1(b)에서, 역 극성(reverse polarity)의 n-형 확산층(20)이 형성되어 p-n 접합부를 형성한다. n-형 확산층(20)은 인 옥시클로라이드 (POCl3)를 인 공급원으로서 사용하여 인 (P)의 열적 확산에 의해 형성될 수 있다. 임의의 특정 변형이 없는 경우, n-형 확산층(20)은 규소 p형 기판의 전체 표면 위에 형성된다. 확산층의 깊이는 확산 온도 및 시간을 제어하여 변화될 수 있으며, 일반적으로 약 0.3 미크론 내지 0.5 미크론의 두께 범위로 형성된다. n형 확산층은 수십 옴/스퀘어의 시트 저항을 가질 수 있다.In FIG. 1 (b), an n-
도 1(c)에 도시된 바와 같이, 레지스트 등을 사용하여 n-형 확산층(20)의 한쪽 표면을 보호한 후 에칭함으로써 대부분의 표면으로부터 n형 확산층을 제거하여 n-형 확산층(20)이 단지 한쪽 주요 표면에만 남아 있게 된다. 이어서, 유기 용매 등을 사용하여 레지스트가 제거된다.As shown in Fig. 1 (c), one surface of the n-
이어서, 도 1(d)에서, 반사방지 코팅으로서 또한 기능하는 절연층(30)을 n-형 확산층(20) 상에 형성한다. 절연층은 보통 질화규소이나 또한 SiNx:H 막(즉, 절연막이 후속 소성 처리 중의 패시베이션(passivation)을 위한 수소를 포함함), 산화티타늄 막, 또는 산화규소 막일 수 있다. 약 700 Å 내지 900 Å 두께의 질화규소 막이 약 1.9 내지 2.0의 굴절률을 위해 적합하다. 절연층(30)의 침착은 스퍼터링, 화학 기상 증착, 또는 다른 방법에 의해 행해질 수 있다.Subsequently, in FIG. 1 (d), an insulating
다음으로, 전극을 형성한다. 도 1(e)에서 도시된 바와 같이, 본 발명의 후막 페이스트 조성물은 절연막(30) 상에서 스크린-인쇄된 다음 건조된다. 또한, 알루미늄 페이스트(60) 및 후면 은 페이스트(70)를 기판의 후면 위로 스크린 인쇄하고, 이어서 건조시킨다. 수 초 내지 수십 분의 기간 동안 750℃ 내지 850℃의 온도에서 소성을 수행한다.Next, an electrode is formed. As shown in Fig. 1 (e), the thick film paste composition of the present invention is screen-printed on the insulating
그 결과로, 도 1(f)에 도시된 바와 같이, 소성 동안, 후면에서는 알루미늄이 알루미늄 페이스트로부터 규소 기판 내로 확산하여, 고농도의 알루미늄 도펀트를 함유하는 p+ 층(40)을 형성한다. 이 층은 일반적으로 후면전계(back surface field, BSF) 층이라고 하며, 태양 전지의 에너지 변환 효율을 개선시키는 데 도움이 된다. 소성은 건조된 알루미늄 페이스트(60)를 알루미늄 후면 전극(61)으로 변환시킨다. 동시에 후면 은 페이스트(70)가 소성되어 은 또는 은/알루미늄 후면 전극(71)이 된다. 소성 동안, 후면 알루미늄과 후면 은의 사이의 경계는 합금 상태를 띠며, 이로 인해 전기 접속부를 성취한다. 알루미늄 전극이 후면 전극의 대부분의 영역을 차지하는데, 이는 p+ 층(40)의 형성에 대한 필요성에 일부 기인한다. 동시에, 알루미늄 전극에 대한 땝납이 불가능하기 때문에, 은 또는 은/알루미늄 후면 전극이 구리 리본 등에 의해 태양 전지를 상호접속시키기 위한 전극으로서 후면의 제한된 영역에 형성된다.As a result, as shown in Fig. 1 (f), during the firing, aluminum diffuses from the aluminum paste into the silicon substrate on the back side, forming a p +
전면 상에서, 본 발명의 후막 페이스트 조성물(500)은 소결되고 소성 동안에 절연막(30)을 통해 침투되어, n-형 확산층(20)과 전기적 접촉한다. 이러한 유형의 방법은 일반적으로 "소성(fire through)"이라고 한다. 이 소성 상태, 즉 페이스트가 용융되고 절연막(30)을 통해 통과하는 정도는 절연막(30)의 질 및 두께, 페이스트의 조성, 및 소성 조건에 좌우된다. 소성될 때, 페이스트(500)는 도 1(f)에서 도시된 바와 같이 전극(501)이 된다.On the front surface, the thick
한 실시 양태에서, 절연막은 산화티타늄, 산화알루미늄, 질화규소, SiNx:H, 산화규소, 규소 탄소 옥시나이트라이드, 탄소를 함유하는 질화규소 막, 탄소를 함유하는 산화규소 막, 및 산화규소/산화티타늄 막으로부터 선택된다. 질화규소 막은 스퍼터링, 플라즈마 화학 기상 증착 (PECVD), 또는 열적CVD 과정에 의해 형성될 수 있다. 한 실시 양태에서, 산화규소 막은 열적 산화, 스퍼터링, 또는 열적 CFD나 플라즈마 CFD에 의해 형성된다. 산화티타늄 막은 반도체 기판 위로 티타늄-함유 유기 액체 물질을 코팅시키고 소성함으로써, 또는 열적 CVD에 의해 형성될 수 있다.In one embodiment, the insulating film includes titanium oxide, aluminum oxide, silicon nitride, SiN x : H, silicon oxide, silicon carbon oxynitride, silicon nitride film containing carbon, silicon oxide film containing carbon, and silicon oxide / titanium oxide Selected from the film. Silicon nitride films may be formed by sputtering, plasma chemical vapor deposition (PECVD), or thermal CVD processes. In one embodiment, the silicon oxide film is formed by thermal oxidation, sputtering, or thermal CFD or plasma CFD. The titanium oxide film can be formed by coating and firing a titanium-containing organic liquid material over a semiconductor substrate, or by thermal CVD.
이 과정에서, 반도체 기판은 단일-결정 또는 다중-결정질 규소 전극일 수 있다.In this process, the semiconductor substrate may be a single-crystal or multi-crystalline silicon electrode.
적합한 절연막은 산화알루미늄, 산화티타늄, 질화규소, SiNx:H, 산화규소, 규소 카본 옥시나이트라이드, 탄소를 함유하는 질화규소 막, 탄소를 함유하는 산화규소 막, 및 산화규소/산화티타늄으로부터 선택되는 하나 이상의 성분을 포함한다. 본 발명의 한 실시 양태에서, 절연막은 반사 방지 코팅(ARC)이다. 절연막은 반도체 기판에 도포될 수 있거나, 산화규소의 경우에서와 같이 자연 발생할 수 있다.Suitable insulating films include one selected from aluminum oxide, titanium oxide, silicon nitride, SiN x : H, silicon oxide, silicon carbon oxynitride, silicon nitride films containing carbon, silicon oxide films containing carbon, and silicon oxide / titanium oxide It contains the above components. In one embodiment of the invention, the insulating film is an antireflective coating (ARC). The insulating film may be applied to the semiconductor substrate, or may occur naturally as in the case of silicon oxide.
한 실시 양태에서, 절연막은 질화규소 층을 포함한다. 질화규소는 CVD (화학 기상 증착), PECVD (플라즈마 화학 기상 증착), 스퍼터링, 또는 다른 방법에 의해 침착될 수 있다.In one embodiment, the insulating film comprises a silicon nitride layer. Silicon nitride may be deposited by CVD (chemical vapor deposition), PECVD (plasma chemical vapor deposition), sputtering, or other methods.
한 실시 양태에서, 절연 층의 질화규소는 질화규소의 일부 이상을 제거하도록 처리된다. 처리는 화학적 처리일 수 있다. 질화규소의 일부 이상의 제거에 의해, 반도체 기판과 후막 페이스트 조성물의 전도체 사이의 전기적 접촉이 개선될 수 있다. 이로써 반도체 디바이스의 효율이 개선될 수 있다.In one embodiment, the silicon nitride of the insulating layer is treated to remove at least a portion of the silicon nitride. The treatment may be a chemical treatment. By removing at least some of the silicon nitride, the electrical contact between the semiconductor substrate and the conductor of the thick film paste composition can be improved. This can improve the efficiency of the semiconductor device.
한 실시 양태에서, 절연막의 질화규소는 반사방지 코팅의 일부이다.In one embodiment, the silicon nitride of the insulating film is part of an antireflective coating.
후막 페이스트 조성물은 예를 들어, 연결선이 있는 부스바와 같은 패턴으로 절연막 위에 인쇄될 수 있다. 인쇄는 스크린 인쇄, 도금, 압출, 잉크젯, 형상 또는 다중 인쇄(shaped or multiple printing), 또는 리본(ribbon)에 의해 수행될 수 있다.The thick film paste composition may be printed on the insulating film, for example, in a pattern such as a busbar with connecting lines. Printing may be performed by screen printing, plating, extrusion, inkjet, shaped or multiple printing, or ribbons.
이러한 전극 형성 과정에서는, 후막 페이스트 조성물을 가열하여 유기 매질을 제거하고 금속 분말을 소결시킨다. 가열은 공기 중에서 또는 산소-함유 분위기에서 수행할 수 있다. 이러한 단계를 보통 "소성"이라고 한다. 전형적으로 소성 온도 프로파일은 건조된 후막 페이스트 조성물로부터 유기 결합제 물질뿐만 아니라 존재하는 임의의 기타 유기 물질의 번아웃(burnout)이 가능하도록 설정된다. 한 실시 양태에서, 소성 온도는 750℃ 내지 950℃이다. 소성은 0.05 분 내지 5분의 홀드-업(hold-up) 시간을 야기하는 높은 수송 속도, 예를 들어, 100 ㎝/분 내지 500 ㎝/분을 사용하여 벨트 화로(belt furnace)에서 수행될 수 있다. 원하는 온도 프로파일을 제어하기 위해 다수의 온도 구역, 예를 들어, 3 개 내지 11 개의 구역이 사용될 수 있다.In this electrode formation process, the thick film paste composition is heated to remove the organic medium and sinter the metal powder. Heating can be carried out in air or in an oxygen-containing atmosphere. This step is commonly referred to as "firing". Typically the firing temperature profile is set to enable burnout of the organic binder material as well as any other organic material present from the dried thick film paste composition. In one embodiment, the firing temperature is between 750 ° C and 950 ° C. Firing can be carried out in a belt furnace using a high transport speed, for example 100 cm / min to 500 cm / min, resulting in a hold-up time of 0.05 to 5 minutes. have. Multiple temperature zones can be used, for example three to eleven zones, to control the desired temperature profile.
소성 시, 전기 전도성 금속 및 Pb-Te-O 혼합물은 절연막에 침투된다. 절연막의 침투로 인해, 전극과 반도체 기판 사이에 전기적 접촉이 형성된다. 소성 후에, 내부층은 반도체 기판과 전극 사이에 형성될 수 있으며, 여기서 내부층은 텔루륨, 텔루륨 화합물, 납, 납 화합물, 및 규소 화합물 중 하나 이상을 포함하고, 규소는 규소 기판 및/또는 절연 층(들) 으로부터 기원할 수 있다. 소성 후, 전극은 하부의 반도체 기판과 접촉하고 또한 하나 이상의 절연 층과 접촉할 수 있는 소결된(sintered) 금속을 포함한다.Upon firing, the electrically conductive metal and Pb-Te-O mixture penetrates into the insulating film. Due to penetration of the insulating film, electrical contact is formed between the electrode and the semiconductor substrate. After firing, an inner layer may be formed between the semiconductor substrate and the electrode, wherein the inner layer comprises one or more of tellurium, tellurium compounds, lead, lead compounds, and silicon compounds, and silicon being a silicon substrate and / or Originating from the insulating layer (s). After firing, the electrode comprises a sintered metal that can be in contact with the underlying semiconductor substrate and can also be in contact with one or more insulating layers.
본 발명의 또 다른 측면은:Another aspect of the invention is:
(a) 반도체 기판의 하나 이상의 표면 위로 침착된 하나 이상의 절연막을 포함하는 반도체 기판을 제공하는 단계;(a) providing a semiconductor substrate comprising one or more insulating films deposited over one or more surfaces of the semiconductor substrate;
(b) 하나 이상의 절연막의 적어도 일부분 위에 후막 페이스트 조성물을 도포하여, 계층화된 구조물을 형성하는 단계,(b) applying a thick film paste composition over at least a portion of the at least one insulating film to form a layered structure,
(여기서, 후막 페이스트 조성물은:Wherein the thick film paste composition is:
i) 조성물 내 총 고형물을 기준으로 85 중량% 내지 99.5 중량%의 전기 전도성 금속 또는 그의 유도체;i) 85 to 99.5 weight percent of the electrically conductive metal or derivative thereof, based on the total solids in the composition;
ii) 고형물을 기준으로 0.5 중량% 내지 15 중량%의 납-텔루륨-산화물 (여기서, 납-텔루륨-산화물의 납 대 텔루륨의 몰 비는 5/95 내지 95/5임); 및ii) 0.5% to 15% by weight of lead-tellurium-oxide based on solids, wherein the molar ratio of lead to tellurium of lead-tellurium-oxide is 5/95 to 95/5; And
iii) 유기 매질을 포함함); 및iii) an organic medium); And
(c) 반도체 기판, 하나 이상의 절연막, 및 후막 페이스트를 소성시키고, 하나 이상의 절연 층과 접촉하고 반도체 기판과 전기적 접촉하는 전극을 형성하는 단계를 포함하는 방법에 의해 형성되는 물품이다.(c) firing the semiconductor substrate, the at least one insulating film, and the thick film paste, and forming an electrode in contact with the at least one insulating layer and in electrical contact with the semiconductor substrate.
그러한 물품은 광기전력 디바이스의 제조에 유용할 수 있다. 한 실시 양태에서, 물품은 후막 페이스트 조성물로부터 형성되는 전극을 포함하는 반도체 디바이스이다. 한 실시 양태에서, 전극은 규소 태양 전지 상의 전면 전극이다. 한 실시 양태에서, 물품은 후면 전극을 추가로 포함한다.Such articles can be useful in the manufacture of photovoltaic devices. In one embodiment, the article is a semiconductor device comprising an electrode formed from a thick film paste composition. In one embodiment, the electrode is a front electrode on a silicon solar cell. In one embodiment, the article further comprises a back electrode.
실시예EXAMPLE
후막 페이스트 조성물의 예시적인 제조 및 평가는 하기에서 기술된다.Exemplary preparations and evaluations of thick film paste compositions are described below.
실시예 IExample I
납-텔루륨-산화물 제조Lead-tellurium-oxide manufacturing
표 1 & 2의 유리 프릿의 납-텔루륨-산화물 제조Lead-tellurium-oxide Preparation of the Glass Frit of Tables 1 & 2
TeO2 분말 (99+% 순도) 및 PbO 분말 (ACS 시약 등급, 99+ % 순도) 및 선택적으로, PbF2, SiO2, B2O3, P2O5, 납 포스페이트, SnO2, SnO, Li2O, Li2(CO3), Li(NO3), V2O5, Ag2O, Ag2(CO3), Ag(NO3)의 혼합물을 폴리에틸렌 용기 내에서 30 분 동안 텀블링하여 출발 분말을 혼합하였다. 출발 분말 혼합물을 백금 도가니에 두고, 공기 내에서 10℃/분의 가열 속도로 900℃로 가열시킨 다음, 900℃에서 1 시간 동안 유지시켜 혼합물을 용융시켰다. 화로로부터 백금 도가니를 제거하고 용융물을 스테인리스 강 압반 위로 부어서 900℃에서부터 용융물을 급랭시켰다. 생성 물질을 막자사발 및 막자에서 100 메시 미만으로 연삭시켰다. 다음, 연삭된 물질을, D50이 0.5 미크론 내지 0.7 미크론이 될 때까지 폴리에틸렌 용기 내에서 지르코니아 볼 및 아이소프로필 알코올을 이용해 볼-분쇄시켰다. 다음, 볼-분쇄된 물질을 분쇄 볼로부터 분리하고, 건조시키고, 100 메시 스크린을 통해 진행시켜 후막 페이스트 제조에 사용되는 플럭스 분말을 제공하였다.TeO 2 powder (99 +% purity) and PbO powder (ACS reagent grade, 99 +% purity) and optionally PbF2, SiO2, B2O3, P2O5, lead phosphate, SnO2, SnO, Li2O, Li2 (CO3), Li ( A mixture of NO3), V2O5, Ag2O, Ag2 (CO3), Ag (NO3) was tumbled in a polyethylene vessel for 30 minutes to mix the starting powder. The starting powder mixture was placed in a platinum crucible and heated to 900 ° C. at a heating rate of 10 ° C./min in air, then held at 900 ° C. for 1 hour to melt the mixture. The platinum crucible was removed from the furnace and the melt was poured onto a stainless steel platen to quench the melt from 900 ° C. The resulting material was ground to less than 100 mesh in the mortar and pestle. The ground material was then ball-milled with zirconia balls and isopropyl alcohol in a polyethylene vessel until D 50 was between 0.5 and 0.7 microns. The ball-milled material was then separated from the grinding balls, dried and run through a 100 mesh screen to provide the flux powder used for thick film paste preparation.
[표 1]TABLE 1
[표 2]TABLE 2
표 3의 유리 프릿의 납-텔루륨-산화물 제조Lead-tellurium-oxide preparation of the glass frit of Table 3
표 3의 납-텔루륨-리튬-산화물 (Pb-Te-Li-Ti-O) 조성물은, Pb3O4 및 TeO2 분말, 및 선택적으로 표 3에서 제시된 바와 같이, SiO2, P2O5, Pb2P2O7, Ag2O, Ag(NO3) 및/또는 SnO2를 혼합하고 블렌딩함으로써 제조하였다. 블렌딩된 분말 배치 물질을 백금 합금 도가니에 로딩한 다음, 공기 또는 O2 함유 분위기를 사용해 900℃ 내지 1000℃에서 화로 내에 삽입하였다. 가열 처리의 기간은 구성분의 전체 용액의 달성 후 20 분 이었다. 다음, 구성분의 융합으로 인한 생성 저 점도의 액체를 금속 롤러에 의해 급랭시켰다. 다음, 급랭된 유리를 분쇄하고, 스크리닝하여 0.1 미크론 내지 3.0 미크론의 D50을 갖는 분말을 제공하였다.The lead-tellurium-lithium-oxide (Pb-Te-Li-Ti-O) compositions of Table 3 are Pb 3 O 4 and TeO 2 powders, and optionally as shown in Table 3, SiO 2 , P 2 O Prepared by mixing and blending 5 , Pb 2 P 2 O 7 , Ag 2 O, Ag (NO 3 ) and / or SnO 2 . The blended powder batch material was loaded into a platinum alloy crucible and then inserted into the furnace at 900 ° C. to 1000 ° C. using an air or O 2 containing atmosphere. The duration of heat treatment was 20 minutes after the achievement of the total solution of the components. Next, the resulting low viscosity liquid due to the fusion of the components was quenched by a metal roller. The quenched glass was then ground and screened to provide a powder with a D 50 of 0.1 micron to 3.0 microns.
[표 3]TABLE 3
실시예 IIExample II
페이스트 제조Paste manufacturer
표 5, 6, 7, & 8의 후막 페이스트 제조Thick Film Paste Preparations in Tables 5, 6, 7, & 8
후막 페이스트의 유기 성분 및 상대적인 양은 표 2에 제공된다.The organic components and relative amounts of the thick film pastes are provided in Table 2.
[표 4]TABLE 4
유기 성분을 틴키 혼합 병(Thinky mixing jar) (틴키 USA, 인크(Thinky USA, Inc)) 내에 넣고 잘 블렌딩될 때까지 2000 RPM에서 2 분 내지 4 분 동안 틴키-혼합하였다. 무기 성분 (Pb-Te-O 분말 및 은 전도성 분말)을 유리 병에서 15 분 동안 텀블-혼합하였다. 무기 성분의 총 중량은 88 g이었고, 이 중 85 g 내지 87 g은 은 분말이었고 1 g 내지 3 g은 PbO 및 TeO2 분말의 혼합물이었다. 다음, 무기 성분 중 1/3을 유기 성분이 든 틴키 병에 첨가하고, 2000 RPM에서 1 분 동안 혼합하였다. 모든 무기 성분이 첨가되고 혼합될 때까지 이를 반복하였다. 페이스트를 냉각시키고, 용매를 첨가한 다음 200 RPM에서 1 분 동안 혼합해서 점도를 200 Pa.s 내지 500 Pa.s로 조정하였다. 원하는 점도가 달성될 때까지 이 단계를 반복하였다. 다음, 페이스트를 0 ㎫ (0 psi)에서 3 회 통과 및 0.52 ㎫ (75 psi)에서의 3 회 통과 동안 0.025 ㎜ (1 mil) 갭에서 롤-분쇄하였다. 분산 정도는 입도계(fineness of grind, FOG)에 의해 측정하였다. FOG 값은 전형적으로 후막 페이스트에 대해 20/10과 동일하거나 미만이다. 각각의 페이스트의 점도는 #14 스핀들(spindle) 및 #6 컵을 이용하는 브룩필드 점도계 상에서 측정하였다. 페이스트의 점도를 실온에서 24 시간 후에 200 Pa.s 내지 320 Pa.s로 조정하였다. 점도는 점도계에서 10 RPM에서 3 분 후에 측정하였다.The organic components were placed in a Tinky mixing jar (Thinky USA, Inc) and tin-mixed for 2-4 minutes at 2000 RPM until well blended. The inorganic components (Pb-Te-O powder and silver conductive powder) were tumble-mixed for 15 minutes in a glass bottle. The total weight of the inorganic components was 88 g, of which 85 g to 87 g were silver powders and 1 g to 3 g were mixtures of PbO and TeO 2 powders. Next, one third of the inorganic component was added to the Tinky bottle with organic components and mixed for 1 minute at 2000 RPM. This was repeated until all inorganic components were added and mixed. Cool the paste, add solvent and mix for 1 minute at 200 RPM to obtain a viscosity of 200 Pa . s to 500 Pa . adjusted to s. This step was repeated until the desired viscosity was achieved. The paste was then roll-milled in a 0.025 mm (1 mil) gap for three passes at 0 psi (0 psi) and three passes at 0.52 MPa (75 psi). The degree of dispersion was measured by a fineness of grind (FOG). The FOG value is typically equal to or less than 20/10 for thick film pastes. The viscosity of each paste was measured on a Brookfield viscometer using a # 14 spindle and a # 6 cup. The viscosity of the paste is 200 Pa after 24 hours at room temperature . s to 320 Pa . adjusted to s. Viscosity was measured after 3 minutes at 10 RPM on a viscometer.
[표 5]TABLE 5
표 9, 10, 12, & 13의 후막 페이스트 제조Thick Film Paste Preparation of Tables 9, 10, 12, & 13
페이스트 제조물은 일반적으로 하기 절차를 사용해 제조하였다: 표 9, 10, 12, & 13의 용매, 매질 및 계면활성제의 적절한 양을 칭량하고, 혼합기 캔 내에서 15 분 동안 혼합하였다.Paste preparations were generally prepared using the following procedure: Appropriate amounts of solvents, media, and surfactants in Tables 9, 10, 12, & 13 were weighed and mixed in a mixer can for 15 minutes.
Ag가 고형물의 대부분이므로, 더욱 우수한 습윤을 보장하기 위해 이를 증분식으로 첨가하였다. 잘 혼합되었을 때, 페이스트를 0에서 1.72 ㎫로 (0에서 250 psi로) 점진적으로 증가하는 압력으로 3-롤 밀에 반복 통과시켰다. 롤들 간의 갭은 0.051 ㎜ (2 밀)로 설정하였다. 페이스트 점도를 브룩필드 점도계를 사용해 측정하였고, 적절한 양의 용매 및 수지를 첨가하여 페이스트 점도가 230 Pa-sec 내지 280 Pa-sec의 표적으로 가게 조정하였다. 분산 정도는 입도계(FOG)에 의해 측정하였다. 페이스트에 대한 전형적인 FOG 값은, 4번째로 긴 연속 스크래치의 경우 20 미크론 미만이고, 페이스트의 50%가 스크래치되는 지점에서는 10 미크론 미만이다.Since Ag is the majority of the solids, it was added incrementally to ensure better wetting. When well mixed, the paste was repeatedly passed through a 3-roll mill at progressively increasing pressure from 0 to 1.72 MPa (0 to 250 psi). The gap between the rolls was set to 0.051 mm (2 mils). Paste viscosity was measured using a Brookfield viscometer and the paste viscosity was adjusted to a target of 230 Pa-sec to 280 Pa-sec by adding the appropriate amount of solvent and resin. The degree of dispersion was measured by particle size (FOG). Typical FOG values for the paste are less than 20 microns for the fourth longest continuous scratch and less than 10 microns at the point where 50% of the paste is scratched.
표 9, 10, 12 & 13의 데이타를 생성하는 데 사용되는 최종 페이스트를 제조하기 위해, 표 1의 프릿 중 2 중량% 내지 3 중량%를 Ag 페이스트 중 일부 내로 혼합하고 당업자에게 뮬러(muller)로서 알려진 회전 유리 판 사이에서 전단에 의해 분산시켰다. 표 12 & 13의 최종 페이스트를 제조하기 위해, 1) 적절한 양의 Ag를 표 4의 적절한 양의 비히클에 첨가하고 롤 분쇄시키고, 2) 표 3의 적절한 양의 제1 유리 프릿을 표 4의 적절한 양의 비히클에 첨가하고 롤 분쇄시키고, 3) 표 3의 적절한 양의 제2 유리 프릿을 표 4의 적절한 양의 비히클에 첨가하고 롤 분쇄시켜서 3 개의 개별 페이스트를 제조하였다. 적절한 양의 Ag 페이스트 및 프릿 페이스트를 행성형 원심분리 혼합기(planetary centrifugal mixer) (일본 도쿄 소재의 틴키 코포레이션(Thinky Corporation))를 사용해 함께 혼합하였다.To prepare the final paste used to generate the data of Tables 9, 10, 12 & 13, from 2% to 3% by weight of the frits of Table 1 were mixed into some of the Ag paste and as a muller to those skilled in the art. Dispersed by shear between known rotating glass plates. To prepare the final pastes of Tables 12 & 13, 1) an appropriate amount of Ag was added to the appropriate amount of vehicle in Table 4 and roll milled, and 2) an appropriate amount of first glass frit from Table 3 was applied in Table 4 Three individual pastes were prepared by adding to the amount of vehicle and rolling mill, and 3) the appropriate amount of second glass frit from Table 3 was added to the appropriate amount of vehicle from Table 4 and roll milling. Appropriate amounts of Ag paste and frit paste were mixed together using a planetary centrifugal mixer (Thinky Corporation, Tokyo, Japan).
표 11은 표 12 및 13의 실시예의 조합된 프릿 조성물을 제시한다. 표 11에서 제시된 조합된 프릿 조성물은 표 12 & 13의 블렌딩 비율로 표 3의 프릿 조성물을 사용하여 계산한다.Table 11 shows the combined frit compositions of the examples of Tables 12 and 13. The combined frit compositions shown in Table 11 are calculated using the frit compositions of Table 3 with the blending ratios of Tables 12 & 13.
표 5, 7, 8, 9, 12, 및 13의 페이스트 실시예는 하기 상세한 설명에 따라 표에서 열거된 페이스트 조성물의 제조에 대한 상기 기술된 절차를 사용하여 제조하였다. 시험된 페이스트는 85% 내지 88%의 은 분말을 함유하였다. 이들 실시예는 D50 = 2.0 ㎛인 단일 구형 은을 사용하였다.Paste Examples of Tables 5, 7, 8, 9, 12, and 13 were prepared using the procedures described above for the preparation of paste compositions listed in the table according to the following detailed description. The tested paste contained 85% to 88% silver powder. These examples used single spherical silver with a D 50 = 2.0 μm.
실시예 IIIExample III
태양 전지 제조Solar cell manufacturing
표 6, 7, & 8의 실시예의 태양 전지 제조Solar Cell Preparation of Examples of Tables 6, 7, & 8
후막 페이스트의 성능을 시험하기 위한 태양 전지는, 65 ohm/sq 인-도핑된 에미터(emitter) 층을 갖는 175 미크론의 두꺼운 Q.셀 다중-결정질 규소 웨이퍼로부터 제조하였고, 이는 산-에칭된 텍스처화된 표면 및 70 ㎚의 두꺼운 PECVD SiNx 반사방지 코팅을 가졌다. 태양 전지는 독일 OT 딸레하임(OT Thalheim, Germany) 소재의 Q-셀즈 SE(Q-Cells SE)에 의해 공급되었다. 웨이퍼를 다이아몬드 웨이퍼링 톱을 사용해 28 ㎜ × 28 ㎜ 웨이퍼로 절단하였다. AMI-프레스코 MSP-485 스크린 인쇄기를 사용해 절단한 후 웨이퍼를 스크린-인쇄하여, 0.254 ㎝ 피치에서 부스바의 11 개의 전도체 라인(line), 및 완전한 지반면(ground-plane)의, 스크린-인쇄된 알루미늄 후면 전도체를 제공하였다. 인쇄 및 건조 후, 전지를 BTU 국제 급속 열 가공 벨트 화로(BTU International rapid thermal processing belt furnace)에서 소성시켰다. 표 3에서 제시된 소성 온도는 화로 설정점 온도였고, 이는 실제 웨이퍼 온도보다 대략 125℃ 더 높았다. 소성된 전도체 라인 중앙 선 폭은 120 미크론이었고 평균 선 높이는 15 미크론이었다. 중앙 라인 저항은 3.0E-6ohm.㎝였다. 28 ㎜ × 28 ㎜ 전지의 성능은 전체 태양 전지 충진 인자(fill factor, FF)를 약 5% 정도 감소시키는 모서리 효과에 의해 영향을 받는 것으로 예상된다.Solar cells for testing the performance of thick film pastes were fabricated from 175 micron thick Q. cell multi-crystalline silicon wafers with 65 ohm / sq phosphorus-doped emitter layers, which were acid-etched textures. It had a hardened surface and a thick PECVD SiN x antireflective coating of 70 nm. The solar cells were supplied by Q-Cells SE of OT Thalheim, Germany. The wafer was cut into a 28 mm x 28 mm wafer using a diamond wafering saw. After cutting using an AMI-FRESCO MSP-485 screen press, the wafers are screen-printed, eleven conductor lines of busbars at 0.254 cm pitch, and complete ground-plane, screen-printed aluminum Provided back conductor. After printing and drying, the cells were fired in a BTU International rapid thermal processing belt furnace. The firing temperatures presented in Table 3 were the furnace set point temperatures, which were approximately 125 ° C. higher than the actual wafer temperature. The fired conductor line center line width was 120 microns and the average line height was 15 microns. Center line resistance is 3.0E-6ohm . Cm. The performance of a 28 mm by 28 mm cell is expected to be affected by the corner effect of reducing the overall solar cell fill factor (FF) by about 5%.
표 9, 10, 12, & 13의 실시예의 태양 전지 제조Solar Cell Preparation of Examples of Tables 9, 10, 12, & 13
p-형 베이스 상에 인-도핑된 에미터를 이용해 2.79 ㎝ × 2.79 ㎝ (1.1" × 1.1") 다이싱-소우-컷(dicing-saw-cut) 다중-결정질 규소 태양 전지에 페이스트를 도포하였다. 실시예 번호 1의 페이스트를 62 Ω/□ 에미터를 갖는 도이체쎌 (독일 소재 도이체쎌) 다중-결정질 웨이퍼에 도포하였고, 실시예 번호 2 내지 6의 페이스트를 55 Ω/□ 에미터를 갖는 긴텍(Gintech) (타이완 소재 긴텍 에너지 코포레이션(Gintech Energy Corporation)) 다중-결정질 웨이퍼에 도포하였다. 사용된 태양 전지는 등방성 산 에칭에 의해 텍스처화되었고, SiNX:H의 반사방지 코팅 (ARC)를 가졌다. 표 9, 10, 12 & 13에서 제시된 바와 같이 효율 및 충진 인자를 각 샘플에 대해 측정하였다. 각각의 페이스트에 대해, 5 개 내지 12 개의 샘플에 대한 효율 및 충진 인자의 평균 및 중앙 값이 제시된다. 250 ㎜/초의 스퀴지(squeegee) 속도로 설정된 ETP 모델 L555 인쇄기를 사용한 스크린-인쇄에 의해 각각의 샘플을 제조하였다. 사용된 스크린은 325 메시 및 23 ㎛ 와이어를 갖는 스크린에서 20 ㎛의 에멀젼으로, 1.5 ㎜ 개구를 갖는 1 개의 부스바 및 100 ㎛ 개구를 갖는 11 개의 핑거 라인의 패턴을 가졌다. 통상적으로 입수가능한 Al 페이스트인, 듀폰(DuPont) PV381을 디바이스의 비조사면 (후면) 위에 인쇄하였다.The paste was applied to a 1.1 "x 1.1" dicing-saw-cut multi-crystalline silicon solar cell using an in-doped emitter on a p-type base. . The paste of Example No. 1 was applied to a Deutsche® (Deutsche®, Germany) multi-crystalline wafer having a 62 Ω / □ emitter, and the pastes of Examples Nos. 2 to 6 were applied to Gintec® having a 55 Ω / □ emitter. Gintech (Gintech Energy Corporation, Taiwan) was applied to multi-crystalline wafers. The solar cells used were textured by isotropic acid etching and had an antireflective coating (ARC) of SiN X : H. Efficiency and filling factors were measured for each sample as shown in Tables 9, 10, 12 & 13. For each paste, the mean and median values of efficiency and filling factors for 5 to 12 samples are shown. Each sample was prepared by screen-printing using an ETP model L555 printer set at a squeegee speed of 250 mm / sec. The screen used had a pattern of 11 finger lines with one busbar with 1.5 mm opening and 100 μm opening with an emulsion of 20 μm in a screen with 325 mesh and 23 μm wire. DuPont PV381, a commonly available Al paste, was printed on the non-irradiated side (back side) of the device.
이어서, 양면 상에 인쇄된 패턴을 갖는 디바이스를 건조 오븐에서 250℃의 피크 온도로 10분 동안 건조시켰다. 이어서, 560 ㎝/분의 벨트 속도 및 550-600-650-700-800-905℃ 내지 945℃ 온도 설정점을 사용하여 CF7214 데스패치(Despatch) 6 구역 IR 화로에서 태양광 면을 위로 하여 기판을 소성하였다. 처리 중에 부품의 실제 온도를 측정하였다. 각 부품의 추정된 피크 온도는 740℃ 내지 780℃였고, 각 부품은 총 4 초의 시간 동안 650℃ 초과였다. 이어서, 완전히 처리된 샘플을, 보정된 ST-1000 테스터를 사용하여 PV 성능에 대해 시험하였다.The device with the pattern printed on both sides was then dried for 10 minutes at a peak temperature of 250 ° C. in a drying oven. Subsequently, the substrate was placed face up in the CF7214 Despatch 6 zone IR furnace using a belt speed of 560 cm / min and a temperature set point of 550-600-650-700-800-905 ° C to 945 ° C. Fired. The actual temperature of the part was measured during the treatment. The estimated peak temperature for each part was 740 ° C. to 780 ° C. and each part was above 650 ° C. for a total of 4 seconds. The fully processed sample was then tested for PV performance using a calibrated ST-1000 tester.
실시예 IVExample IV
태양 전지 성능: 효율 및 충진 인자Solar Cell Performance: Efficiency and Filling Factors
시험 절차: 표 6, 7, & 8의 실시예에 대한 효율 및 충진 인자Test Procedures: Efficiency and Filling Factors for the Examples of Tables 6, 7, & 8
태양 전지 성능을 ST-1000, 텔레콤 STV Co. IV 테스터를 사용해 25℃ +/- 1.0℃에서 측정하였다. IV 테스터에 있는 제논 아크 램프는 알려진 강도의 태양광을 시뮬레이션하였고, 전지의 전면에 조사하였다. 테스터는 전지의 I-V 곡선을 결정하기 위해 대략 400 부하 저항 설정으로 전류(I) 및 전압(V)을 측정하기 위해 4-접촉 방법을 사용하였다. 태양 전지 효율(Eff), 충진 인자(FF), 및 직렬 저항(Rs)을 I-V 곡선으로부터 계산하였다. Rs는 특히 접촉 저항(ρc), 전도체 라인 저항 및 에미터 시트 저항에 의해 영향을 받는다. 전도체 라인 저항 및 시트 저항은 통칭 다양한 샘플에 대해 동등하였기 때문에, Rs의 차이는 주로 ρc로 인한 것이었다. Suns-VOC 기법을 사용해 이상 계수를 측정하였다. 이상 계수는 0.1 태양 방사조도(sun irradiance)에서 보고된다.Solar cell performance ST-1000, Telecom STV Co. Measurement was made at 25 ° C. +/− 1.0 ° C. using an IV tester. A xenon arc lamp in the IV tester simulated sunlight of known intensity and irradiated the front of the cell. The tester used a four-contact method to measure current (I) and voltage (V) at approximately 400 load resistance settings to determine the I-V curve of the cell. Solar cell efficiency (Eff), fill factor (FF), and series resistance (Rs) were calculated from the I-V curve. Rs is particularly affected by the contact resistance ρ c, the conductor line resistance and the emitter sheet resistance. Since conductor line resistance and sheet resistance were generally equivalent for various samples, the difference in Rs was mainly due to ρc. The anomaly coefficients were measured using the Suns-VOC technique. The anomaly coefficient is reported at 0.1 sun irradiance.
실시예 1 내지 12의 후막 페이스트를 사용하여 제조된 태양 전지에 대한 효율, 충진 인자, 직렬 저항, 및 이상 계수의 중앙 값을 측정하였고, 표 6에서 요약한다. 실시예 13 내지 27의 틴크-막 페이스트를 사용하여 제조된 태양 전지에 대한 효율의 평균 및 중앙 값을 측정하였고, 표 7에서 요약한다. 실시예 13 내지 27의 틴크-막 페이스트를 사용하여 제조된 태양 전지에 대한 충진 인자의 평균 및 중앙 값을 측정하였고, 표 8에서 요약한다.The median values of efficiency, fill factor, series resistance, and anomaly coefficients for the solar cells prepared using the thick film pastes of Examples 1-12 were measured and summarized in Table 6. The average and median values of the efficiency for the solar cells prepared using the tin-film pastes of Examples 13-27 were measured and summarized in Table 7. The average and median values of the fill factors for solar cells prepared using the tink-membrane pastes of Examples 13-27 were measured and summarized in Table 8.
[표 6]TABLE 6
[표 7]TABLE 7
[표 8]TABLE 8
시험 절차: 표 9, 10, 12, & 13의 실시예에 대한 효율 및 충진 인자Test Procedures: Efficiency and Filling Factors for the Examples of Tables 9, 10, 12, & 13
본 명세서에 기술된 방법에 따라 구성된 태양 전지를 변환 효율에 대해 시험하였다. 예시적인 효율 시험 방법을 하기에 제공한다.Solar cells constructed according to the methods described herein were tested for conversion efficiency. An exemplary efficiency test method is provided below.
한 실시 양태에서, 본 명세서에 기술된 방법에 따라 구성된 태양 전지를 효율 측정용의 시판의 I-V 테스터 (텔레콤 STV, 모델 ST-1000)에 넣었다. I-V 테스터 내의 제논 아크 램프는 알려진 강도로 태양광을 시뮬레이션하였고, 전지의 전면에 조사하였다. 테스터는 다점 접촉 방법을 사용해 대략 400 부하 저항 설정에서 전류(I) 및 전압(V)을 측정하여 전지의 I-V 곡선을 결정하였다. I-V 곡선으로부터 충진 인자(FF)와 효율(Eff) 둘 모두를 계산하였다.In one embodiment, solar cells constructed according to the methods described herein were placed in a commercial I-V tester (Telecom STV, Model ST-1000) for efficiency measurement. A xenon arc lamp in an I-V tester simulated sunlight at a known intensity and irradiated the front of the cell. The tester determined the I-V curve of the cell by measuring the current (I) and voltage (V) at approximately 400 load resistance settings using the multipoint contact method. Both fill factor (FF) and efficiency (Eff) were calculated from the I-V curve.
[표 9]TABLE 9
[표 10]TABLE 10
[표 11]TABLE 11
[표 12]TABLE 12
[표 13]TABLE 13
비교예 I: 비스무스-텔루륨-산화물Comparative Example I: Bismuth-tellurium-oxide
비스무스-텔루륨-산화물의 제조Preparation of Bismuth-Telium-Oxide
표 14에서 제시된 바와 같은 비스무스-텔루륨-산화물 (Bi-Te-O) 함유 조성물을, 산화붕산 (B2O3), 산화아연 (ZnO), 산화티타늄 (TiO2), 비스무스 산화물 (Bi2O3), 산화텔루륨 (TeO2), 탄산리튬 (LiCO3), 및 인산리튬 (LiPO4)를 사용해 실시예 I: 표 3의 유리 프릿의 납-텔루륨-산화물 제조에서 상기 기술된 절차에 의해 제조하였다.The bismuth-tellurium-oxide (Bi-Te-O) containing composition as shown in Table 14 was prepared by boric acid (B 2 O 3 ), zinc oxide (ZnO), titanium oxide (TiO 2 ), bismuth oxide (Bi 2). Example I: Procedure described above in the preparation of lead-tellurium-oxide of the glass frit of Table 3 using O 3 ), tellurium oxide (TeO 2 ), lithium carbonate (LiCO 3 ), and lithium phosphate (LiPO 4 ) Prepared by.
[표 14]TABLE 14
페이스트 제조Paste manufacturer
유리 A를 사용한 페이스트를 하기 절차에 의해 제조하였다. 적절한 양의 유기 비히클 (표 4) 및 Ag 분말을 혼합하여 페이스트를 제조하였다. Ag 페이스트를 0 ㎫에서 0.52 ㎫로 (0 psi에서 75 psi로) 점진적으로 증가하는 압력으로 3롤 밀을 통해 통과시켰다. Ag 페이스트 점도를 브룩필드 점도계를 사용해 측정하였고, 적절한 양의 용매 및 수지를 첨가하여 페이스트 점도가 230 Pa-sec 내지 280 Pa-sec의 표적으로 가게 조정하였다. 적절한 양의 유기 비히클 (표 4) 및 유리 분말 A를 혼합하여 또 다른 페이스트를 제조하였다. 프릿 페이스트를, 0 ㎫에서 1.72 ㎫ (0 psi에서 250 psi)로 압력을 점진적으로 증가시키면서 3-롤 밀을 통해 통과시켰다. 각각의 페이스트의 분산 정도를 입도계 (FOG)에 의해 측정하였다. 페이스트에 대한 전형적인 FOG 값은, 4번째로 긴 연속 스크래치의 경우 20 미크론 미만이고, 페이스트의 50%가 스크래치되는 지점에서는 10 미크론 미만이다.Paste using Glass A was prepared by the following procedure. A paste was prepared by mixing the appropriate amount of organic vehicle (Table 4) and Ag powder. Ag paste was passed through a three roll mill at progressively increasing pressure from 0 MPa to 0.52 MPa (0 psi to 75 psi). Ag paste viscosity was measured using a Brookfield viscometer and the paste viscosity was adjusted to a target of 230 Pa-sec to 280 Pa-sec by addition of the appropriate amount of solvent and resin. Another paste was prepared by mixing the appropriate amount of organic vehicle (Table 4) and glass powder A. The frit paste was passed through a 3-roll mill with gradual increase in pressure from 0 MPa to 1.72 MPa (250 psi at 0 psi). The degree of dispersion of each paste was measured by particle size (FOG). Typical FOG values for the paste are less than 20 microns for the fourth longest continuous scratch and less than 10 microns at the point where 50% of the paste is scratched.
Ag 및 프릿 페이스트를 행성형 원심분리 혼합기 (일본 도쿄 소재의 틴키 코포레이션)를 사용해 함께 혼합시키면서 혼합하여, 표 15에서 나타낸 최종 페이스트 레시피를 제조하였다.Ag and frit paste were mixed while mixing together using a planetary centrifugal mixer (Tinky Corporation, Tokyo, Japan) to prepare the final paste recipe shown in Table 15.
테양 전지 제조 및 효율과 충진 인자 측정Manufacture of Teyang Battery and Measurement of Efficiency and Filling Factor
p-형 베이스 상에 인-도핑된 에미터를 이용해 2.79 ㎝ × 2.79 ㎝ (1.1" × 1.1") 다이싱-소우-컷 다중-결정질 규소 태양 전지에 페이스트를 도포하였다. 페이스트를 62 Ω/□ 에미터를 이용해 도이체쎌 (독일 도이체쎌 사 제품) 다중-결정질 웨이퍼에 도포하였다. 사용된 태양 전지는 등방성 산 에칭에 의해 텍스처화되었고, SiNX:H의 반사방지 코팅 (ARC)을 가졌다. 표 15에서 제시된 바와 같이 효율 및 충진 인자를 각각의 샘플에 대해 측정하였다. 200 ㎜/초의 스퀴지 속도로 설정된 ETP 모델 L555 인쇄기를 사용한 스크린-인쇄에 의해 각각의 샘플을 제조하였다. 사용된 스크린은 325 메시 및 23 ㎛ 와이어를 갖는 스크린에서 20 ㎛의 에멀젼으로, 1.5 ㎜ 개구를 갖는 1 개의 부스바 및 100 ㎛ 개구를 갖는 11 개의 핑거 라인의 패턴을 가졌다. 통상적으로 입수가능한 Al 페이스트인, 듀폰 PV381을 디바이스의 비조사면 (후면) 상에 인쇄하였다.The paste was applied to a 1.1 "by 1.1" dicing-saw-cut multi-crystalline silicon solar cell using an in-doped emitter on the p-type base. The paste was applied to a Deutsche® multi-crystalline wafer from Deutsche GmbH, Germany, using a 62 Ω / □ emitter. The solar cells used were textured by isotropic acid etching and had an antireflective coating (ARC) of SiN X : H. Efficiency and filling factors were measured for each sample as shown in Table 15. Each sample was prepared by screen-printing using an ETP model L555 printer set at a squeegee speed of 200 mm / sec. The screen used had a pattern of 11 finger lines with one busbar with 1.5 mm opening and 100 μm opening with an emulsion of 20 μm in a screen with 325 mesh and 23 μm wire. DuPont PV381, a commonly available Al paste, was printed on the non-irradiated side (back side) of the device.
이어서, 양면 상에 인쇄된 패턴을 갖는 디바이스를 건조 오븐에서 250℃의 피크 온도로 10분 동안 건조시켰다. 다음, 560 ㎝/분의 벨트 속도 및 500-550-610-700-800-HZ6 온도 설정점을 사용하여 CF7214 데스패치 6 구역 IR 화로에서 태양광 면을 위로 하여 기판을 소성시켰고, 여기서 HZ6은 885℃, 900℃ & 915℃였다. 처리 중에 부품의 실제 온도를 측정하였다. 각 부품의 추정된 피크 온도는 745℃ 내지 775℃였고, 각각의 부품은 총 4 초의 시간 동안 650℃ 초과였다. 다음, 완전히 처리된 샘플을, 보정된 ST-1000 테스터를 사용하여 PV 성능에 대해 시험하였다.The device with the pattern printed on both sides was then dried for 10 minutes at a peak temperature of 250 ° C. in a drying oven. The substrate was then fired with the solar face up in the CF7214 Despatch 6 Zone IR furnace using a belt speed of 560 cm / min and a 500-550-610-700-800-HZ6 temperature set point, where HZ6 was 885 ° C, 900 ° C & 915 ° C. The actual temperature of the part was measured during the treatment. The estimated peak temperature for each part was 745 ° C. to 775 ° C. and each part was above 650 ° C. for a total of 4 seconds. The fully processed sample was then tested for PV performance using a calibrated ST-1000 tester.
표 15에서 제시된 효율 및 충진 인자를 각각의 샘플에 대해 측정하였다. 각각의 페이스트에 대해, 6 개의 샘플에 대한 효율 및 충진 인자의 평균 및 중앙 값이 제시된다.The efficiency and filling factors shown in Table 15 were measured for each sample. For each paste, the mean and median values of efficiency and filling factors for six samples are shown.
[표 15]TABLE 15
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KR20060108547A (en) * | 2005-04-14 | 2006-10-18 | 이 아이 듀폰 디 네모아 앤드 캄파니 | Method of manufacture of semiconductor device and conductive compositions used therein |
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